Process of converting massive and other forms of sulphur into finelydivided flowers of sulphur



Dec. 2, I1924. 1,518,126

C. J. PROCESS OF CONVERTING MASSIVE AND OTHER FORMS OF SULPHUR INTOFINELY DIVIDED FLOWERS OF SULPHUR l Filed Aug. 1, 1925 Q u n Y\I F* j so w g i u a-mi N X m. u 'u w Y (3 N kgn g L\. L L w Patented Dec. 2,1924.

CHARLES J'. REED, OF SAN MATEO, CALIFORNIA, ASSIGNOR. OF ONE-HALF T0ALICE A.

HALL OF SAMN'FRANCISCO, CALIFORNIA. f

PROCESS F OONVERTINGf MASSIVE AND OTHER FORMS OF SULPHUR INTO' FINELY-DIVIDED FLOWERS 0F SULPHUR.

Appication led ug'ust 1, 1923. Serial No. 655,110.

To all whom t may concern.'

Be it known that I, CHARLES J. REED, a

citizen of the United States, residing at San Mateo, in the county ofSan Mateo and State of California, have invented new and usefulImprovements in Processes of Converting Massive and Other Forms ofSulphur into Finely-Divided Flowers of Sulphur, of which the followingis a specicaton.

My invention relates to the producing of owers of sulphur. I accomplishthis object by the process herein described, which consists invaporizing any form of sulphur by heating it in a closed receptacle ofany form to a temperature above the boiling point of sulphur, about 445degrees C., "diluting this vapor or gaseous sulphur withoutreducing itstemperature by injecting into it an inert gas, or mixture of inert gasespreviously heated to a temperature not lower than the boiling point ofsulphur, and subsequently projecting into the diluted gaseous mixture apreviously cooled inert gas or gaseous mixture in sufficient quantity toreduce the temperature of the sulphur vapor below 115 degrees C., thevmelting point of sulphur. This solidifes the sulphur particles while themass is diluted and thereby produces only minute particles of solidsulphur.

- In the ordinary process of making flowers of sulphur the sulphur isvaporized and the undiluted vapor is projected into a condensingchamber, where it gradually cools and condenses, first to liquid drops,which afterwards solidify. In hat process theundiluted vapor condensesto liquid particles which, on account of their proximity andgreatconcentration into small volume, collect into comparatively largemasses while still liquid. These large liquid masses on solidifying formlarge solid crystalline masses, most of them too large'to be classed asflowers of sulphur.

In my improved process the dilution of the sulphur vapor beforecondensation by mixing it with a large quantity of previously heatedinert grs separates the particles of sulphur vapor by increasing thedistances between them and distributing them uniformly through a largervolume. Under these conditions the subsequent cooling and condensingproduces only minute particles of liquid and solid sulphur. The

minuteness obtainable by this process is limited only by the amount ofdilution' before reduction of temperature, that is, before there is anycondensation of the liquid or solid state. y

My process may be carried out in any suitable form of apparatus, one ofwhich is shown in the accompanying drawing. But I am not limited to themechanism -or arrangements shown, and it is largely diagrammatic incharacter and proportions, but, if constructed in accordance withthedrawing, would be entirely operative.

Inthe drawing 1 represents a retort or vaporizing chamber heated by anysuitable source'of heat, 2. A vertical, tubular inlet, 3, `is for theintroduction of sulphur, 23, from the hopper, 33, and valve, 24. A shortpipe, 5, connects the retort with a heater, 6, having a source of heat,7. Y- The heater, 6, is for preheating a portion of the circulatinggases before their introduction into the vapor of sulphur. A tubularoutlet, 4, for the transportation of heated gases and vapor of sulphur,leads from the retort to the condensing chamber, 8. Into this condensingchamber containing the hot, diluted sulphur vapor, cooled inert gas isprojected from the tubular chamber, 9, through the tubular nozzles, 10.A trough, 11, below the A the vapor to nozzles, 10, is for the purposeof catching` any liquid sulphur whichmay condense on the' nozzles, 10,and fall down. A'tube, 12, leads from the condensing chamber,8, to thesettling tank,v 13, suitably arranged to collect the minute flowers ofsulphur formed inv 8. A series of conical outlets, 14, is for the exitof the flowers of sulphur formed in 8. Asimilar series of outlets, 15,is for that which collects in 13. A blower, 16, is for maintaining Ithecirculation of the gases in the direction indicated by arrows. The tube,17, conveys the gases from the blower, 16, into 18 and 19. The tubes,18, and 19, convey portions of the circulating gas to the cooler, 22,and the heater, 6, respectively, A sliding door or diaphragm, 21,movable in a closely fitting slot, in the wall of the tube, 18, isadapted to regulate the flow of gases in the cooler, 22. A similar door,20, in the tube, 19, regulates the flow of gases to the heater, 6. Eachof the conical outlets, 14 and 15, is provided with a tacle.

close-fitting door or a close-hitting recep- Such 'a door is shown inthe dra-W- ing at the bottom ot each outlet. lEach door comprises acover, 26, articulated by ahinge, 27, to a support, 28, and is held upby a re- .tractile spring, 29. The gas cooler, 22,'comlprises a coolingcoil of pipe, 25, having terminals, 3l and 32,l and inclosed in' thechamber, 22. @ne of the terminals, 31er 32, is connectedx to a source ofsupply of cold' Water, not shown in the drawing. The heater, 6,comprises a number of vertical tubes, 34, through Which the products ofcombustion pass' trom the burners, 7. 'lhe gases to be heated loW aroundthe tubes, 34, into the retort, 1, as indicated by arrows. A shelf orwhich with the residual nitrogen and vapor other internal receptacle,35, in the cold chamber, 9, is for holding a desiccator or otherchemical reagent. movable stopper, 36, closes an opening above thisshelf.

ln my improved process ll prefer to introduce lime or other active basicchemical reagent into thel gaseous circuitto absorb oxides ot sulphurand other gases Which may be present and detrimental to the product.

ll prefer nitrogen as a circulating mediunn,

though a mixture of nitrogen and sulphur dioxide operatessatisfactorily.

llhe` entire apparatus is protected from loss of heat by the insulatingcovering, 30.

Thecovers of the outlets, 14 and l5, are.

to prevent the inux of air, but may be opened for the outlovv ofsulphur.

lln the operation of my process ll introduce sulphur, 23, in any form,solid or liquid, into the retort, l, by raising the valve, 24. rlheblovver, 16, is set in operation, causing a continuous circulation ofthe air Within the closed system, as indicated by arrovvs, 'lhe burners,2 and 7, are set in operation and cold Water, or other cooling agent, iscaused to low from a source not shown in the drawing through thev coil,25, ci the cooler. When( the temperature in the retort and in theheater, `6, exceeds 445 to 448 degrees C., vapor oi sulphur formed inthe retort and mixed vvith the heated ain-is oxidized to sulphurdioxide,

of Sulphur passes through the tube, 4, into the condensing chamber, 8.The tube, 4, must be `Well insulated and the temperature of the mixedgases from the retort and heater must be maintained above the boilingpoint of sulphur, to prevent condensation of sulphur in the tube, 4. lprefer a temperature or at least 460 C. ln a short time all oxygenoriginally contained in the system is converted into sulphur dioxide andthe circulating gas is then a mixture of nitrogen and sulphurdioxide.The sulphur dioxide may be, but need not necessarily be, absorbed bylime or other basic active chemical reagent. The mixture of nitrogen andsulphur dioxide, or the nitrogen alone, or the nitrogen mixed with argonand Whatever medium about ten times the volume or proportions andoperating at the temp 0gastarse 'should be cooled to as low atemperature as may be convenient and economical. llt flows aftercooling-through the tubular chamber,

9, and the nozzles, l0, into the condensing chamber, 8, mixing with the-superheated and diluted vapor of sulphur and condensing it to minutesolid crystals. ,lhe introduction of the superheated circulating mediuminto the vapor of sulphur at or in the retort, or inthe tube, 4,leading'rom the retort, is very important and is one oit the essentialsteps in my process. lits purpose is to dilute the sulphur vapor Withoutcondensing it, thus causing the atoms or molecules of gaseous sulphur toseparate to greater distances apart and to become separated byintervening particles of other inert, nor-- condensible gases. Afterthis separation of the molecules ot sulphur vapor by intervening inertgaseous particles has been accomplished While the sulphur remains in thegaseous state, it is then possible by proper cooling to condense theindividual separated sulphur molecules to the solid state and producethe finest possible llovvers ot sulphur. llt, however, the undilutedvapor of sulphur be cooled and condensed, as is done in methodsheretofore employed, the particles olf sulphur in condensing to theliquid state will, on account ot then' proximity and the absence oit anyother intervening inert gaseous particles, collect together intocomparatively large liquid drops, which on solidiying will formcomparatively large crystalline masses.

ll am not limited to any particular proporice tions in the gaseousmixture, but pret-er to dilute the hot sulphur vapo-r by about ten timesits volume of the superheated circulating medium. yllhis mixture passesthrough the heatedtube, 4, into the condensing chamber, 8. lnto thiscondensing cham.-

vber and into the diluted vapor of sulphur is also-projected through thenozzles, l0, a cold portion of the circulating medium coming trom4 thecooler, 22, through the tubular chamber, 9. l prefer to inject ot coldsuperheated mixture, and prefer to have cold medium at a temperature nothigher than about fortyA degrees C. With tures above mentioned l rindthat practica t all of the sulphur vapor is condensed tne solid state inexceedingly small particles. I,

A portion of the condensed ilovvers ol" phur formed in the chamber, 8,lah bottom of the chamber and are collected the outlets,l4, but largeportion is carried by the circulating medium through the tube, 12, intothe settlin tank, 13, where it collects and is removed tlrough theoutlets, 15.

l claim:

1. The process of producing flowers 'of sulphur, which consists invaporizing the sulphur at a Itemperature not lower than the boilingpoint of sulphur,`1nixing the vapor of sulphur withan inert gaseouscirculating medium also at a temperature not less than the boiling pointof sulphur, and subsequently mixing these products with an'inert gaseouscirculatingI medium at a lower temperature.

2. The process of producing flowers of sulphur, which consists invaporizing the sulphur at a temperature not lower than the boilingtemperature of sulphur, mixing the vapor of sulphur with an inert gas ata temperature not less than the boiling temperature of sulphur, andsubsequently mixing the product with an inert gas at a temperature lowerthan the fusing temperature of sulphur.

3. An apparatus vfor producing flowers of sulphur, comprising avaporizing chamberor vaporizing sulphur, a heating chamber adapted toheat a portion of a gaseous circulating medium, a cooling chamberadapted to cool a portion of a gaseous circulating medium, a condensingchamber adapted to receive the heated and cooled portions of a gaseouscirculating medium, and a blower adapted to circulate a gaseous medium,all connected into a closed system, substantially ask herein set forth.

CHARLES J. REED;

